CN112624753B - 基于450nm光固化制备极小曲面复杂结构氧化锌陶瓷的方法 - Google Patents

基于450nm光固化制备极小曲面复杂结构氧化锌陶瓷的方法 Download PDF

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CN112624753B
CN112624753B CN202011075459.XA CN202011075459A CN112624753B CN 112624753 B CN112624753 B CN 112624753B CN 202011075459 A CN202011075459 A CN 202011075459A CN 112624753 B CN112624753 B CN 112624753B
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赵艳
陆嘉雄
曾勇
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Beijing University of Technology
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Abstract

基于450nm光固化制备极小曲面复杂结构氧化锌陶瓷的方法涉及3D打印技术领域，使用三维设计软件Rhino 6设计出所需的极小曲面模型，改变壁厚以及形状等方式，调控孔隙率，使用Magics软件对导出模型进行修复优化，并以STL的格式导入进光源为450nm的商用陶瓷DLP 3D打印机器中，按照特定比例，配置出适合的陶瓷浆料，并且进行球磨，真空消泡处理后，设置合适的打印参数进行打印制备胚体，打印结束后酒精清理，并进行脱脂烧结，得到可应用于过滤吸附，太赫兹吸收等应用的高孔隙率极小曲面氧化锌陶瓷。

Description

基于450nm光固化制备极小曲面复杂结构氧化锌陶瓷的方法
技术领域
本发明涉及3D打印技术及功能陶瓷制备、环境治理、以及微波吸收应用领域，特别是使用了DLP(数字光固化)3D打印技术制备了具有良好力学性能，质量轻的可用于微波吸收以及过滤吸附的极小曲面复杂结构氧化锌陶瓷。
背景技术
ZnO是一种带隙宽度为3.3ev的半导体材料，具有良好的压电特性、热电效应、抗菌等性能。它耐高温。因此，ZnO陶瓷被广泛应用于微波吸收、抗菌、换热、避雷针等各个领域。随着工业的发展，人们对高性能陶瓷的要求越来越高，这就对陶瓷零件的结构和尺寸精度提出了更高的要求。最近，人们的兴趣转向了具有最小表面特征的基于壳的拓扑，如三层周期极小小曲面(TPMS)和各向异性的随机旋向最小曲面等。有文献指出极小曲面结构没有节点和其他应力强化区域，从而提高了强度和韧性，并在低压降下实现了有效的流体输送。遗憾的是，传统的陶瓷成型方法和加工方法无法制造出极小曲面复杂结构的陶瓷。为了实现高精度的极小曲面状复杂结构氧化锌陶瓷，本发明将传统陶瓷制造工艺与3D打印技术相结合，利用DLP光固化打印技术制备极小曲面状氧化锌陶瓷，再通过传统的脱脂烧结方法，制备成功极小曲面复杂结构氧化锌陶瓷。目前在市场上尚未有适合450nm光波长固化的ZnO陶瓷浆料售卖，也没有查到适用于lithoz LITHOZ CeraFab 7500的450nm光固化ZnO浆料文献与专利。
发明内容
本发明的目的是提供一种基于450nm光固化制备极小曲面复杂结构氧化锌陶瓷的方法。
1)使用三维建模软件设计极小曲面结构，根据有限元分析软件ANSYS的力学模拟结果，对极小曲面结构薄壁的厚度进行调整，最终得到70％-90％孔隙率的极小曲面复杂结构模型，并以STL格式导出；
2)450nm光固化浆料配置：
对氧化锌粉末进行球磨至粒径小于等于500nm；
38wt％氧化锌纳米粉末、3wt％1,6-hexanediol diacrylate(HDDA)作为粘结剂，4wt％的三乙醇胺作为分散剂，1wt％正硅酸乙酯作为助烧结剂，49wt％季戊四醇三丙烯酸酯作为树脂，2.5wt％2,4,6-樟脑醌和2.5wt％4-二甲氨基苯甲酸乙酯作为450nm光引发剂，按比例混合，然后搅拌；
然后加入氧化锆珠，在行星球磨机中进行球磨，以250r/min的速度进行球磨，持续180min，彻底混合得到浆料；将浆料装入容器，放入真空干燥机进行真空消泡处理；
3)3D打印制备过程：
将需要打印的极小曲面复杂结构的CAD模型以STL格式输入到商用陶瓷DLP3D打印机器中，用于打印的的光固化波长为450nm,层厚设置为0.025mm,单层曝光时间2s；参数设置以及调平完成，随即开始打印；
4)脱脂与烧结过程
打印完成后，从成形板取下进行后处理；用高压气枪将极小区面结构表面和内部的残余浆液冲洗出来，再使用酒精清理打印完成后的坯体；然后将洗净的坯体放置在中号烧结炉中，在高温下对样品进行脱脂以去除有机物，脱脂环节设置如下：
室温25℃，升温至300℃，升温速率为1.5℃/min，保温时间90min；300℃升温至500℃，升温速率1.2℃/min，保温时间60min；500℃升温至600℃，升温速率0.5℃/min，保温时间90min；600℃升温至900℃，升温速率1.5℃/min，保温时间90分钟；900℃降温至室温25℃，降温速率2℃/min；
B.烧结环节：
升温温度为1280℃，升温速度为2℃/min；
保温时间为2.5h，降温至室温，降温速率为2℃/min。
对烧结后的极小曲面氧化锌陶瓷成品进行了表面形貌观察以及力学性能分析等试验。SEM图显示，晶粒致密，无明显的裂纹和团聚。力学性能优异，可用于环境污染吸附、以及微波吸收等应用领域。
本方法具有以下创新性：
(1)本发明首次自主制备了可用于固化光波长为450nm的DLP 3D打印的氧化锌陶瓷浆料，流动性好，稳定性高。
(2)本发明首次使用DLP技术打印出了极小曲面的氧化锌陶瓷(ZnO)，其所使用的原材料为450nm波段光敏树脂。
(3)本发明探究出了基于455nm光固化制备极小曲面氧化锌陶瓷的成型工艺以及烧结工艺参数，得到成型率高，力学性能优异，质量轻的极小曲面氧化锌陶瓷
附图说明
图1是Schwarz P极小曲面结构，
图2是Gyroid极小曲面结构。
图3是实例一中Schwarz P极小曲面结构3D打印坯体的立体形貌图
具体实施方式
将需要打印的极小曲面复杂结构的CAD模型以STL格式输入到商用陶瓷DLP3D打印机器(CeraFab 7500，LITHOZ)中，对仪器进行清洗，基板调平以及设置参数，用于打印的的光固化波长为450nm,层厚设置为0.025mm,单层曝光时间2s。参数设置以及调平完成后，随即开始打印。
打印完成后，用小铲子将胚体从成形板取下进行后处理。用高压气枪将极小区面结构表面和内部的残余浆液冲洗出来，再使用酒精进行冲洗清理。放入真空干燥箱中干燥20h，然后将洗净的坯体放置在日本岛电FP93中号炉中，在高温下对样品进行脱脂以去除有机物，并且进行烧结。过程如下：
A.脱脂过程：
室温25℃，升温至300℃，升温速率为1.5℃/min，保温时间90min；300℃升温至500℃，升温速率1.2℃/min，保温时间60min；500℃升温至600℃，升温速率0.5℃/min，保温时间90min；600℃升温至900℃，升温速率1.5℃/min，保温时间90分钟；900℃降温至室温25℃，降温速率2℃/min；
B.烧结环节：
升温温度为1280℃，升温速度为2℃/min；
保温时间为2.5h，降温至室温，降温速率为2℃/min。
实例一：
1.使用犀牛Rhino 6等三维建模软件设计极小曲面Schwarz P，Gyroid，曲面生成公式分别为cos(x)+cos(y)+cos(z)＝0，cos(x)sin(y)+cos(x)sin(z)+cos(y)sin(z)＝0，并改变其胞壁的厚度，从而设计其孔隙率皆为为85％。
2.以300r/min的速度对氧化锌粉末进行球磨，持续300min，把38wt％氧化锌纳米粉末、3wt％1,6-hexanediol diacrylate(HDDA)作为粘结剂，4wt％的三乙醇胺(TEA)作为分散剂，1wt％正硅酸乙酯作为助烧结剂，49wt％季戊四醇三丙烯酸酯作为树脂，3wt％2,4,6-樟脑醌和3wt％4-二甲氨基苯甲酸乙酯作为450nm光引发剂，按比例混合，然后搅拌。然后加入氧化锆珠，在行星球磨机中进行球磨，以250r/min的速度进行球磨，持续180min，彻底混合。将浆料装入容器，放入真空干燥机进行真空消泡处理。
3.将需要打印的极小曲面复杂结构的CAD模型以STL格式输入到商用陶瓷DLP 3D打印机器(CeraFab 7500，LITHOZ)中，用于打印的的光固化波长为450nm,层厚设置为0.025mm,单层曝光时间2s。参数设置以及调平完成，随即开始打印。
4.打印完成后，从成形板取下进行后处理。用高压气枪将极小区面结构表面和内部的残余浆液冲洗出来，再使用酒精清理打印完成后的坯体。然后将洗净的坯体放置在烧结炉中，在高温下对样品进行脱脂以去除有机物，烧结形成致密的氧化锌陶瓷成品。

Claims (2)

1.一种基于450nm波段光固化成形的极小曲面状氧化锌陶瓷的制备方法，其特征在于：
1）使用三维建模软件设计极小曲面结构，根据有限元分析软件ANSYS的力学模拟结果，对极小曲面结构薄壁的厚度进行调整，最终得到70%-90%孔隙率的极小曲面复杂结构模型，并以STL格式导出；
2）450nm光固化浆料配置：
对氧化锌粉末进行球磨至粒径小于等于500nm；
38wt%氧化锌纳米粉末、3wt% 1,6-己二醇二丙烯酸酯作为粘结剂，4wt%的三乙醇胺作为分散剂，1wt%正硅酸乙酯作为助烧结剂，49wt% 季戊四醇三丙烯酸酯作为树脂，2.5wt%2,4,6-樟脑醌和2.5wt% 4-二甲氨基苯甲酸乙酯作为450nm光引发剂，按比例混合，然后搅拌；
然后加入氧化锆珠，在行星球磨机中进行球磨，以250 r/min的速度进行球磨，持续180min，彻底混合得到浆料；将浆料装入容器，放入真空干燥机进行真空消泡处理；
3）3D打印制备过程：
将需要打印的极小曲面复杂结构的CAD模型以STL格式输入到商用陶瓷DLP 3D打印机器中，用于打印的光固化波长为450nm,层厚设置为0.025mm,单层曝光时间2s；参数设置以及调平完成，随即开始打印；
4）脱脂与烧结过程
打印完成后，从成形板取下进行后处理；用高压气枪将极小区面结构表面和内部的残余浆液冲洗出来，再使用酒精清理打印完成后的坯体；然后将洗净的坯体放置在中号烧结炉中，在高温下对样品进行脱脂以去除有机物，脱脂环节设置如下：
室温25℃，升温至300℃，升温速率为1.5℃/min，保温时间90min；300℃升温至500℃，升温速率1.2℃/min，保温时间60min；500℃升温至600℃，升温速率0.5℃/min，保温时间90min；600℃升温至900℃，升温速率1.5℃/min，保温时间90分钟；900℃降温至室温25℃，降温速率2℃/min；
B．烧结环节：
升温温度为1280 ℃，升温速度为2 ℃/min；
保温时间为2.5 h，降温至室温，降温速率为2 ℃/min。
2.根据权利要求1所述的方法，其特征在于：所使用的3D打印机是商业陶瓷打印机LITHOZ CeraFab 7500，使用建模软件为Rhino 6、Materialise 3-matic 11.0或Magics。
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114455972B (zh) * 2022-02-15 2023-02-03 吉林大学 一种复杂构型近净成型金属-陶瓷复合材料的制备方法
CN116283310B (zh) * 2023-02-16 2024-06-07 山东大学 一种基于光固化3d打印极小曲面结构硅氧烷前驱体陶瓷的方法
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Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1253767A (zh) * 1998-08-20 2000-05-24 可乐丽股份有限公司 牙用粘合剂组合物
JP2007115656A (ja) * 2005-09-26 2007-05-10 Asahi Kasei Chemicals Corp 酸化亜鉛系透明導電性基板の製造方法
CN104194267A (zh) * 2014-08-26 2014-12-10 太仓碧奇新材料研发有限公司 纳米氧化锌基3d打印用光电材料及其制备方法
CN105566860A (zh) * 2015-12-11 2016-05-11 上海联泰科技股份有限公司 一种用于3d光固化成型打印的陶瓷材料及其制备方法
CN106810215A (zh) * 2017-01-18 2017-06-09 深圳摩方新材科技有限公司 一种陶瓷浆料的制备及3d打印光固化成型方法
CN107032798A (zh) * 2017-05-31 2017-08-11 清华大学 一种基于光固化快速成型的多孔陶瓷材料的制备方法
CN107032797A (zh) * 2017-05-31 2017-08-11 清华大学 一种基于光固化成型的陶瓷基层间复合材料及其制备方法
CN107500736A (zh) * 2017-09-15 2017-12-22 华中科技大学 一种用于光固化成型的陶瓷膏体及其制备方法
CN109400177A (zh) * 2018-10-30 2019-03-01 西安点云生物科技有限公司 用于3d光固化成型打印的陶瓷材料及陶瓷制件的制备方法
CN110272273A (zh) * 2019-07-22 2019-09-24 上海应用技术大学 3d打印的可控多孔羟基磷灰石生物陶瓷支架及制备方法
WO2020059399A1 (ja) * 2018-09-21 2020-03-26 株式会社トクヤマデンタル 光硬化性組成物及び義歯床用裏装材、並びにこれらを調製するためのキット

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1253767A (zh) * 1998-08-20 2000-05-24 可乐丽股份有限公司 牙用粘合剂组合物
JP2007115656A (ja) * 2005-09-26 2007-05-10 Asahi Kasei Chemicals Corp 酸化亜鉛系透明導電性基板の製造方法
CN104194267A (zh) * 2014-08-26 2014-12-10 太仓碧奇新材料研发有限公司 纳米氧化锌基3d打印用光电材料及其制备方法
CN105566860A (zh) * 2015-12-11 2016-05-11 上海联泰科技股份有限公司 一种用于3d光固化成型打印的陶瓷材料及其制备方法
CN106810215A (zh) * 2017-01-18 2017-06-09 深圳摩方新材科技有限公司 一种陶瓷浆料的制备及3d打印光固化成型方法
CN107032798A (zh) * 2017-05-31 2017-08-11 清华大学 一种基于光固化快速成型的多孔陶瓷材料的制备方法
CN107032797A (zh) * 2017-05-31 2017-08-11 清华大学 一种基于光固化成型的陶瓷基层间复合材料及其制备方法
CN107500736A (zh) * 2017-09-15 2017-12-22 华中科技大学 一种用于光固化成型的陶瓷膏体及其制备方法
WO2020059399A1 (ja) * 2018-09-21 2020-03-26 株式会社トクヤマデンタル 光硬化性組成物及び義歯床用裏装材、並びにこれらを調製するためのキット
CN109400177A (zh) * 2018-10-30 2019-03-01 西安点云生物科技有限公司 用于3d光固化成型打印的陶瓷材料及陶瓷制件的制备方法
CN110272273A (zh) * 2019-07-22 2019-09-24 上海应用技术大学 3d打印的可控多孔羟基磷灰石生物陶瓷支架及制备方法

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